Process and apparatus for producing industrial oxygen



July 31, 1945; w. L. D E BAUFRE 2,380,417

I PROCESS AND APPARATUS FQR PRODUCING INDUSTRIAL OXYGEN I Filed'Sept. 9;,1941 2 Sheets-Sheet 1 INVENTOR July 1945 w,. DE BAUFRE 2,380,417v

, PROCESS AND APPARATUS FOR PRODUCING INDUSTRIAL OXYGEN Filed Sept. 9, 1941 2 Sheets-Sheet 2 F1642 JNVENTOR Patented ,July 31 1945 rnocnss AND arrsiia'rus FOR Paonucmc mnus'mm OXYGEN I William Lane De Baufre, Lincoln, Nebr. I Application September 9,1941, Serial No. 410,150 I I 19 Claims (01.- lie-175.5) This invention relates to plants for producing I 4 oxygen for industrial purposes.

When industrial. oxygen is required for cutting and particularly for welding, the oxygen to produce such highpurity oxygen, will produce nitrogen of a purity ot about 95 per cent or less. The oxygen carried oil in the nitrogen therefore equals 20 ,per cent or more of the oxygen in the atmospheric air processed. That is, the yield of oxygen is 80 per. cent or less of the oxygen priginally in the air processed when high purity oxygen is produced.

When industrial oxygen is used for enriching atmospheric air blown into a. blast iumace for making pig iron, lower oxygen purity is satisfac iory although slightly more'oxygen is required oi. the lower purity to attain the sameenrichment.

When the purity of the oxygen produced in an .air separation plant is lowered, the nitrogen 'purty is raised. This means that less oxy en is lost in the nitrogen. Consequently, the yield of oxygen is increased in the lower purity oxygen 1 product for the sanie amount of atmospheric air processed. By raising the nitrogen purity to 99' portions of a plant to produce high purity oxygen with the maximum corresponding yield are diilerent' from the proportions of a plant to produce high yield of oxygen with the maximum corresponding purity.

The principal objective of the present invention is to provide means'in an air separation plant to change from the production of oxygen per cent, the yield of oxygen is increased t 95 per cent.

The investment cost and the operating expense oi an air separation plant are dependent mainly upon the quantity of air processed and are affected but slightly by the purities of the oxygen and nitrogen produced. Consequently, the higher the yield oi oxygen, the lower is the cost of oxygen produced i'or'enrichment purposes and other industrial purposes for which a reduced oxygen purity is satisfactory.

An oxygen plant designed and built to produce high purity oxygen, can be operated to produce lower purity oxygen withhigher yield merely by changing the ratio of the rates of withdrawal of the oxygen and nitrogen products. I! this is done. however; the oxygen purity is greatly re- -r'uced', generally to less than 90 per-cent. when he ni rogen. purity is raised to 99 per cent with an oxygen yield of 95 per cent.

An'ongen purity of 95 to 96 per cent with ayield of 95 per cent can be obtained in an oxygen plant pro ortioned for th purpose. If this oxysen plant were operated. however, to produce oxygen of a purity of 99.5 cent; the yield of oxyg n would be very low, due to the low purity 01' nitrogen produced. The yield would be much with high purity and maximum corresponding yield to the production of oxygen with high yield and maximum corresponding purity.

When an oxygen, plant designed and built to produce high purity oxygen, is operated to produce high puritynitrogen with reduced oxygen purity, the operating conditions in the first or preliminary stage of rectification are changed as well as those in the second or final stage of rectification. Less liquid nitrogen is throttled from the first stageto serve as liquid reflux in the second stage in order that this liquid reflux will be nitrogen 01' higher purity and thereby produce the high purity desired in the nitrogen product of the second stage. .liminary rectifieris so constructed that the conditions of operation in the first stage -can be changed by the operator so as to vary the purity of the liquefied nitrogen vapor withdrawn therefrom. This, however, places within the manual control of the operator, a' variable which affects .the ei'iiciency oi operation of the oxygen plant. In the hands of an unskillful operator, the efiiciencyma-y be materially reduced.

Another objective of the present invention is in provide means in an air separation plant to change from high purity oxygen to high yield of oxygen ,without changing the operating co' n- I ditions in-the preliminary rectification.

When the same amo ts oi liquefied high purity nitrogen and of o gen-rich liquid are withdrawn from the preliminary rectifier, it becomes possible to so design the preliminary rectifier that the operation of the whole plant becomes largely automatic, thereby reducing the attention necessary by the operator.

A further object of theihvention is to render the operation of an oxygen plant largely automath: and to arrange the plant so that the oper ation will be mostefllcient under all conditions If the piantis to be operat d to produce high purity nitrogen as well as nitrogen of lower with high purity OXYBen. the liquid reflux in the final rectifier must be sumciently pure to produce the highest purity nitrogen productdesired.

11 conditions in the preliminary rectifier are to remain constant. the final rectifier must be pro- Ordinarily, the prer H The expanded and throttled air enter preliminary rectifier D as-shown." The liquid fraction" drops into pot it at the lower end of preliminaryrectifier D whilethe'vap'or fraction of the entering air-rises through trays 11.; Trays are con-. so structed as described and claimed in U. 8. Patent 1,956,495, issued April 24, -1934. The outside can be assembled and then inserted intogth'e rectifier shelL. The group of trays rests onfland is 4 to prevent 2 V e portioned to produce low purity nitrogen product in spite of the high purity liquid nitrogen'refiux when high purity oxygen isproduced.

Another object of the invention is to obtain 1' s,sso,417;.

liquid reflux for rectifying the rising vapor from the entering atmospheric air into nitrogen yapor of high purity, 99 per cent or better, an oxygen-rich liquid whichaccumulates in pot a high purity oxygen product with high' purity With an eiilcient.preliminaryjrectifier and proper liquid nitrogen reflux in the final rectifier.

In order to obtain the. highest possible yield of "oxygen with the least possible reduction in oxygen purity, -advantag'e1'nust, be taken of all arrangements which will increase refiuxes in boththe preliminary and final rectifiers. Another object'of the invention is to take advantag of all possible heattransfei's for increasing refluxes inthe process.

These' objects and'such other advantages as may hereinafter appear or are incident to the invention, are realized bythe method and apparatus shown in preferred forms on the accompanying drawings.

This invention applies, particularly to two- '20 stage plants as shown in Figure 1 andin Figure 2 for rectifying atmospheric air into oxygen and nitrogen products. the diflerences between 1 these two preferred forms of the invention are in detailsonly, the following descriptionmay be read on both'figures except where one figure is specifically mentioned.

Atmospheric air to be processed enters pipe I at about atmospheric temperature and c0m= pressed to a pressure of 300 to 600 lb. per sq. in.

This compressed air has been freed of carbon dioxide in. scrubbing'tower not shown. If the compressed air has not been dehydrated, inter- .changers A are provided in multiple, so that one interchanger may be defrosted while the remainplained later.

ing interchangers are cooling the compressed air processed. The compressed air is cooled in inter-- changer A to a temperature below minus 100 centigrade as it passes up and around tubes 2- pressed air is expanded ,with performance of external work to a still lower temperature. L'Ihe.

smaller part of the cooled compressed air flows throughpipe 5 into liquefier C where his liqueir. t transfer to the o y and t g n-s0 ,ber. 1.1936. This oxygen-rich liquid is dis-.

products returning through tubes 6. The lique-' fled air is discharged through pipe I and is throttled through valve] into exhaust pipe-I from expansio'n engine 3 or directly into preliminary rectifier D.

diameter of'trays is less than the inside diameter of shell I in .order that a group of trays fastened to a} ring support I) attached to shell i2. Tl'ie-edgeof the topmost tray has a larger uiem ter so that it fits tightly within shell. '1: leakage between thetra'ys the; 70

shell. i Vapor from the topmost tray enters tubes II otyaporiser E where the vapor is partly conproportions of the whole apparatus, this oxygenrich liquid isv nearly in phase equilibrium with v the entering atmospheric air at the same time I that nitrogen vapor of 99 per cent or better leaves the topmost" 'tray' in preliminary rectiller D. 1 V v IrDFigure 1, the nitrogen vapor, from trays l l in preliminary rectifier D flows up through tubes tification due to counterfiow of rising vapor and down-flowing liquid. The. nitrogen leaving through pipe. l'| is therefore of higher purity than the nitrogen vapor rising'from trays H. In Figure 2, the nitrogen vapor flows up through pipe is and'then down through tubes [5 so that "there is no further rectification due to counter- .fiow of vapor and liquid within these tubes. The'nitrogenleaving through pipe IT in Figure 2 is therefore of substantially the same purity as the nitrogen vapor rising from trays II. In this case, a vapor seal I 6 must be provided for the condensed nitrogen returning to trays II as a liquid reflux.

In Figure 2, the vapor remaining unliquefied from vaporizer E passes directly from pipe i! to tubes llwithin condenser F. From tubes II, the vapor still remaining uncbndensed passes over tubes [9 in exchanger G which are cooled by the nitrogen product of the final rectification as ex- In Figure l, the nitrogen from pipe it passes over tubes is in exchanger G before the .vapor flows up-through tubes il in condenser F. In both densible under the-existing pressure and'temperature. In both figures, practically all of the high purity nitrogenvapor from the preliminary rectification is liquefied and collects in pot 2| at the. bottom of condenser F.

I'he oxygen-rich liquid accumulated in pot is at the bottom of preliminary rectifier D is automatically withdrawn by trap 22,.as described and :claimed-inIU. S. Patent- 2;062,781, issued Decemcharged through valve 23 or through valve 24 intojfinal rectifier H. If discharged through rated pipe 25 at about the middle point of final rectifier H with about .an equal number of trays above and --.,below the inlet. If discharged through valve, the oxygen-rich liquid fiows to perforated pipe 2! at a point about one-fourth to. one-third of the total-number of trays from the top of final rectifier H. The trays in the main rectifier are-arranged inthree groups 21,

-28 and", respectively, Each group of trays is arranged as previously described'for group of trays H in preliminary rectifier D.

.65 Reflux liquid for final rectifier H is furnished by the high purity nitrogen liquid which collects v in not 2| at the bottom of condenser F. Ibis nitrogen liquid is automatically withdrawn by trap II and flows through .pipe 8| to vessel 82 within the top of final rectifier H. The high purity. nitrogen liquid from pot'ti is infected into .82 in orderthat vapor may separate therefrom without disturbing the nitrogen prod- I 5 where its purity is improved by further recfigures, a small quantity of fgas' iswithdrawn through valve 2|! to prevent nitrogen pr d- 0 accumulation of any as which-is non-condensed. The? resulting liquidfiows down 5 v not r :the final rectification. The nitrogen through .trays llofpreliminary D as-a 'il liquid flows through vapor. seals u to the top- 2,880,417 most tray in group 29. The separated nitrogen I vapor flows through holes in the walls of vessel 32 and joins the nitrogen product of rectification which leaves through pipe 34.

The oxygen-rich liquid entering final rectifier H through perforated tube 25 or 28 is rectified by trays 21, 28 and 29 into a nitrogen vapor product and an oxygen liquid product. The nitrogen vapor product leaves final rectifier H through pipe 34. This nitrogen product fiows through tubes IS in exchanger G where the nitrogen vapor is warmed somewhat in condensing nitrogen vapor from the preliminary rectification. In 'both figures, the resulting icondensed nitrogen augments the nitrogen liquid in but 2! of condenser F, thereby increasing the liquid nitrogen reflux in the final rectification.

The nitrogen product of the final rectification fiows through the tubes in liquefier C and in interchanger A where the nitrogen product is warmed nearly to the temperature of the atmospheric air entering pipe I, when the nitrogen product leaves through pipe 35.

Liquid oxygen from final rectifier H fiows through pipe. to the space surrounding tubes l-I within vaporizer E. Here the liquid oxygen is partly vaporized in condensing nearly pure nitrogen vapor from preliminaryrectifier D to form liquid reflux for the preliminary rectification. The resulting oxygen vapor returns through pipe 31 to final rectifier H where it forms the vapor reflux for the final rectification. The remaining liquid oxygen flows from vaporizer E through pipe 38 to the space surrounding tubes It in condenser F. Here the vaporization of the liquid oxygen is completed and the resulting oxygen vapor leaves through pipe 40; Pipe 39 equalizes the pressures in vaporizer E and condenser F by permitting flow of vapor in either direction.

With the pressure equalized in vaporizer E and condenser F, the liquid oxygen will rise to substantially the same level in both vaporizer E and condenser F. The heat transfer surfaces in vaporizer E and condenser F consist of vertical tubes extending between lower and upper tube sheets. By having the two lower tube sheets at the same level, the tubes will be submerged equally in liquid oxygen in vaporizer E and condenser F. Hence, as the liquid level varies in vaporizer E during operation of the plant, the heat transfer surfaces in vaporizer E and condenser F will be submerged in a substantially constant ratio. As only the submerged surface of these tubes is very effective in heat transfer from the boiling oxygen liquid to the nitrogen vapor condensing therein, the amounts of nitrogen liquified in vaporizer E and condenser F will be maintained in a substantially constant ratio as the liquid level varies. As the oxygen-rich liquid which accumulates in pot III at the bottom of preliminary rectifier D is about equal tothe amount of liquid nitrogen reflux from vaporizer E, it follows that this construction maintains nearly constant proportions of oxygen-rich liquid and nitrogen liquid accumulating in pots l0 and 2| respectively. This makes possible'the use of automatic means 22 and 30 to discharge these liquids into final rectifier H.

The oxygen product of the final rectification returns from pipe 40 through the tubes in liquefier Cand interchanger A where the oxygen product is warmed nearly to the temperature of the atmospheric air entering pipe I when the oxygen product leaves through pipe 4|.

The valves on outlet pipe 35 for returning and opens valve 23 the other inlet.

of oxygen and nitrogen withdrawn from final' rectifier H. When less oxygen and more nitrogen are withdrawn from any air separation plant, the purity of the oxygen increases and the purity of the nitrogen decreases. When this is done in the present plant, the operator closes valve 23 and opens valve 2| so that the oxygen-rich liquid from pot Iii will enter final rectifier H through pipe 26 rather than through pipe 25, thereby obtaining the greatest yield possible of high purity oxygen. When more oxygen and less nitrogen are withdrawn from any air separation plant, the purity of' the oxygen decreases and the purity of the nitrogen increases. When this is done in the present plant, the operator closes valve 24 so that the oxygen-rich liquid from pot ID will enter final rectifier H through pipe 25 rather than through pipe 26, thereby obtaining the highest purity possible of oxygen with high yield of oxygen.

I claim: I

1. Process of separating atmospheric air into oxygen and nitrogen products which includes separating the atmospheric air into high purity nitrogen vapor and oxygen-rich liquid, liquefying the high purity nitrogen vapor, rectifying the oxygen-rich liquid, with the liquefied high purity nitrogen as liquid reflux into an oxygen product and a nitrogen product, producing vapor refiux for the said rectification by vaporizing liquid oxygen resulting therefrom, providing a. number of intimate contacts of risingvapor and downfiowing liquid in thesaid rectification both above and below the point of introduction of the oxygen-rich liquid whereby a given yield ofoxygen product is produced with a purity corresponding to the relative amounts of oxygen and nitrogen products withdrawn from the process, and changing the ratio of intimate contacts above and below the point of introduction of the oxygen-rich liquid with the same total number of intimate contacts whereby the yield of the oxygen product is changed with a changed purity corresponding to the relative amounts of oxygen and nitrogen products withdrawn from the process.

2. Process of separating atmospheric air into oxygen and nitrogen products as in claim 1 wherein the ratio of. oxygen-rich liquid to liquefied high purity nitrogen from the'preliminary separation remains substantially constant.

3. Apparatus for separating atmospheric air into oxygen and nitrogen products including preliminary means for separating the atmospheric air into high purity nitrogen vapor and oxygenrich liquid, a condenser for liquefying the high purity nitrogen vapor, a final rectifier for rectifying the oxygen-rich liquid with the liquefied high purity nitrogen as liquid reflux into an oxygen product and a nitrogen product, an'inlet at a certain level for the oxygen-rich liquid, a. number of trays. within the' final rectifier disposed partly above and partly below said inlet, a second 'inlet for the oxygen-rich liquid at a. different level with. respect to which said trays are differently disposed, and means for. changing from one to 4. Apparatus for separating atmospheric air into oxygen and nitrogen products which includes preliminary means for separating the atmospheric air into oxygen-rich liquid and nitrogen vapor, a condenser for liquefying the nitrogen vapor, at final rectifier for-rectifying the oxygenrich liquid with the liquefied nitrogen as liquid I por separated from the liquid.

into oxygen and nitrogen products which includespreliminary means for separating the atmospheric air into oxygen-rich liquid and nitrogen vapor with a purity of 99 per. cent or better, a

condenser for liqueiying the nitrogen vapor, a

final rectifier with one inlet for the oxygen-rich liquid to rectify it with the liquefied nitrogen as reflux into an oxygen product over 99 per cent pure and a nitrogen product of lower purity and another inlet at a diiierentlevel to rectify it into a nitrogen product at least 99 per cent pure with reduced oxygen purity, and means for changing from one to the other inlet for the oxygen-rich liquid into the final rectifier in combination with means for varying the rates oi withdrawal of oxyen and nitrogen products therefro 6. Apparatus for separating atmospheric air into oxygen and nitrogen products which includes preliminary means for separating the atmospheric air into oxygen-rich liquid and nitrogen vapor, a condenser for liquefying the nitrogen vapor, a final rectifier for rectifying the oxygenrich liquid with the liquefied ni n as liquid reflux into an oxygen product and a nitrogen product, ,said final rectifier containing trays divided into three groups, and means for introducing the oxygen-rich liquid at either of the -two points of division between the three groups of trays. I

7. Apparatus for separating atmospheric air into oxygen and nitrogen products as in claim 6 wherein the final rectifier has a shell larger in diameter than said trays, and each group of trays rests-on a support attached to said shell with the topmost tray enlarged to fit, tightly into said shell. 8. A rectifier having a shell and groups of trays with an outside diameter less than the inside diameter of said shell,-each group of trays resting on a support attached to said shell with the topmost tray enlarged to fit tightly into said shell. 9. A rectifier as in claim 8 wherein the inlet for the fluid to be rectified is a, perforated pipe extending across said shell between groups of trays.

10. Arectifier as in claim 8 including an inlet for liquid reflux and a vessel .at the top of said shell with a vapor seal for the overflow of liquid refiux to said groups 01' trays and outlets for va- 11. Apparatus for separating atmospheric air into oxygen and nitrogen products including a preliminary rectifier for rectifying the atmospheric air into high purity nitrogen vapor and oxygen-rich liquid, a condenser for liquefying the highpurity nitrogen vapor, a final rectifier-for rectifying the oxygen rlch liquid with the liquefied high purity nitrogen as liquid reflux into an oxygen product ands nitrogen product, a vapor- .izer for vaporizing liquid oxygen from the final rectifier in liquefying high purity nitrogen vapor from the. preliminary rectifier to produce liquid reflux therein, means for admitting liquid oxygen into the condenser and vaporizing it in liqueiying high purity nitrogen vapor with about the same oxygen liquid level in the condenser as in reflux into an oxygen .product and'a nitrogen the vaporizer, the heat transfer surfaces in condenser and vaporizer being disposed so that the ratio of the heating surface areas submerged in liquid oxygen in condenser and vaporizer remains substantiallyconstant with varying oxygen liquid level whereby the ratio of oxygen-rich liquid accumulating in the preliminary rectifier and liquefied high purity nitrogen accumulating in the condenser remains substantially constant, in combination with two inlets for the oxygen-rich liquid'into the final rectifier at difi'erent levels and means for changing from one inlet to the other inlet.

12. Apparatus for separating atmospheric air into oxygen and nitrogen products as in claim 11 wherein means are provided to discharge automatically as rapidly as they accumulate, the oxygen-rich liquid from the preliminary rectifier and the liquefied nitrogen from the condenser.

13. Apparatus for separating atmospheric air into oxygen and nitrogen products including a preliminary rectifier for rectifying the atmospheric air into high purity nitrogen vapor and oxygen-rich liquid, a condenser for liquefying the high purity nitrogen vapor, a finalrectifier for rectifying the oxygen-rich liquid with liquefied high purity nitrogen as liquid reflux into an oxygen product and a nitrogen product, a vaporizer for vaporizing liquid o ygen from the final rectifier in liquefying high puritynitrogen vapor from the preliminary rectifier to produce liquid refiux therein, said vaporizer being arranged for counterflow of rising nitrogen vapor and downflowing nitrogen liquid whereby the purity of the nitirogen vapor is increased before liquefying it in the condenser, in combination with two inlets 1 for the oxygen-rich liquid into the final rectifier at diflerent levels and means for changing from one inlet to the other inlet.

14. Apparatus for separating atmospheric air into oxygen and nitrogen products as in claim 13 including an exchanger for liqueiying high purity nitrogen vapor from said vaporizerby warming the nitrogen product from the final rectifier and means for commingling the liquefied nitrogen from the exchanger with liquefied nitrogen from the condenser, thereby increasing the liquefied nitrogen reflux in the final rectifier and raising the purity of said nitrogen product.

15. Apparatus for separating a gaseous mixture including a preliminary rectifier for rectifying the gaseous mixture into a nearly pure vapor and an impurefliquid, a'final rectifier for rectifying the impure liquid into a vapor product and a liquid product, a vaporizer for producing vapor reflux for the final rectifier and liquid reflux for the preliminary rectifier by partly vaporizing the liquidrproduct of the final rectifier and partly liquefying nearly pure vapor from the preliminary rectifier, a condenser for producing liquid reflux for the final rectifier by liquefying nearly pure vapor from the preliminary rectifier in completing the vaporization of the liquid product of "i-fthe final rectifier, an exchanger for liquefying 6 5,

nearly pure vapor from the preliminary rectifier by warming the vapor product of the final rectifier, the saidexchanger comprising multiple tubes through which the said vapor product flows in heat exchange with said nearly pure vapor surrounding the tubes, and means for commingling liquefied vapor rrom the exchanger with liquefied" vapor from the condenser whereby the liquid reffiux is augmented in the final rectifier.

16. Apparatus for separating, gaseous mixture as in claim 15 wherein means are provided aeedeiv to. convey the nearly pure vapor from thevapor- I izer to the exchanger and thence to the condenser.

1'1. Apparatus for separating a gaseous mixture as in claim 15 wherein the exchanger is mounted above the condenser, the shell oi the exchanger forms a continuation of the shell oi the condenser the tubes extend between a single oompartment at their lower ends and two compartments at their upper ends, and means areprovided for the vapor product to enter one upper compartment and to leave the other upper com-4 partment whereby the vapor product flows down through halt the tubes and up through the other half.

18. A column for separating atmomherlc air into an oxygen product and a nitrogen product comprising a lower group or trays forming a preliminary rectifier for rectifying the atmospheric air into a nitrogen vapor and an oxygen-rich liq uid, multiple upper. groups of trays forming a final rectifier for rectiiying the oxygen-rich aid with liqueiiednitrogen vapor into the oxyg product and the nitrogen product, an intermediate vaporizer tor vaporizing the oxygen product of the final rectiiier in iiquefvins nitrogen vapor from the preliminary rectiiier,- and means for introducing the oxygen-rich liquid from the preliminary rectifier between diflerent groups i of trays in the 'iinal rectifier whereby nearly pure oxygen is obtained with reduced purity nitrogen or nearly pure nitrogen is obtained with reduced purity oxylen.

19. A column for separating atmospheric air into an oxygen product and a nitrogen product as in claim 18 ,wherein the final rectifier contains three groups of trays of which the lowest group contains about the same number of trays as bothupper groups together. 4

' LANE DE BAUI 'RE. 

